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THE REACTION OF CALCIUM CARBIDE 
AND FERRIG OXIDE 


BY 


ISADORE FINKELSTEIN 


THESIS 


FOR THE 


DEGREE OF BACHELOR OF SCIENCE 


IN 


CHEMISTRY 


COLLEGE OF LIBERAL ARTS AND SCIENCES 


UNIVERSITY OF ILLINOIS 
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UNIVERSITY OF ILLINOIS 


2.2 May 30, 192m 


SPS Orme wRTIRY THAT THE DHESIS PREPARED UNDER MY SUPERVISION BY 


Isadore Finkelstein 


eve PROVED BY MEAS FULFILLING THIS PART OF THE REQUIREMENTS FOR THE 


DEGREE OF BACHELOR OF SCIENCE 


Instructor in Charge 


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ACKNOWLEDGMENT 


The writer wishes to express his appreciation and 


Sincere thanks to Dr. W. S. Putnam for his assistance in 


the experimental work and writing of this thesis. 


Digitized by the Internet Archive 
in 2015 


https://archive.org/details/reactionofcalciu0Ofink 


TABLE OF CONTENTS 


Introduction 


Historical 


Experimental 


Conclusions 
Note 
Bibliography 


2 in /. ‘Me on Res es 


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SVMATHOD’ GO BR es 


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INTRODUCTION 


This work was done in connection with that of W. J. 
Farrel on the Desulphurization of steel by calcium carbide. 
The purpose of the work to be described was to determine 
whether or not calcium carbide will react as a reducing agent 
in case oxides were present in the steel and to what degree 
the reduction is carried out. S&. Cohen has done work on the 
reaction of calcium carbide and ferrous sulfide. The results 
of the men mentioned above along with the results obtained in 
this paper may be considered as one, and thus give a compre- 
hensive report on the effects of calcium carbide as a desul- 
phurizing and deoxidizing agent. The great need in the steel 
industry, is a method to eliminate sulphur and phosphorus 
from steel without the electric furnace temperatures. The 
conditions of the investigation do not duplicate those of the 
open hearth furnace, but it was undertaken with the hope of 


learning something more than is mown about the chemical 


activity of Cals that could be applied in making steel. 


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HISTORICAL 


Calcium Carbide was first detected by WShler in 1862. 


On heating a Ca-Zn alloy with carbon at a high temperature he 


obtained a hard substance with a metallic luster, which be- 


came grey on exposure to the atmosphere. The discovery of 


Calcium Carbide is usually accredited to Moisson, who prepared 


it in an electric furnace. He heated coal and calcium oxide 


at temperatures up to about 2000 degrees C and obtained the 


The carbide is formed according to the equation 


carbide. 


given below: 


CaO 4 3C = CaCo + CO 


The present day manufacture of Calcium Carbide is 


according to the equaltion given above. The carbon is in the 


form of finely powdered coal. Care is taken that the coal 


This is necessary in order to 


is of Low sulphur content. 


prevent formation of hydrogen sulfide when the carbide is used 


for the preparation of acetylene gas. The first and largest 


use for the carbide is in the production of acetylene. 


CaCz 4 H20 = CoH, + Ca(OH). 


Calcium carbide according to Erlwein, (1) Wrath and 


Bentner will decompose very slowly. These men did extensive 


work on the decomposition of the carbide by heat. Their re- 


sults show that when CaCy is heated to 1000° C slow decompos- 


ition takes place. They did not identify the product formed, 


but assumed it to be a subcarbide of calcium. No metallic 


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calcium could be detected. On treatment with water no acety- 


lene was evolved, but when nitrogen was passed over the 


material the compound CaCN» was formed. They showed that after 


heating CaCy for 10 hours at 1000°C the carbide analyzed 


36.6% CaCz whereas the sample to start with was 72% CaC,. They 


also noted that NaCl, CaCl and iron powder aided in the de- 


composition of the carbide. When CO gas is passed over CaCy 


at temperatures between 200-250°C, there is a reaction taking 


Dlace as indicated 


Gae> 40 = Cag + 3c 


At 1600°C this reaction is reversible. It may be well 


to note here that according to this equation the carbide must 


be formed at high temperatures. 


Since my problem is one of a reducing nature, it may 


be well to summarize the work that has been done along this 


line. As early as 1899 we find Tarugi (2) worked on the re- 


ducing properties of calcium carbide. He reduced copper 


oxide at bright red heat and the chloride of copper at about 


400°c. Kigelgen (3) has done extensive work on the reducing 


properties of calcium carbide. He worked with the oxides of 


2D, Cu, Ag, Zn, He, Sn, As, W, Mn, Fe, Ni, Al. 


If a mixture as indicated by the equation below is 


heated to dull red heat a reduction takes Place as indicated: 
(1) Poo + CaCo = Pb + CaO 4 2C 


At dull red heat the carbon, which is the graphitic 


form will react as indicated: 


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(2) 4PbO + 2C = 4Pb 4+ 2005 

If the charge contains an excess Of oxide it will re- 
act according to equation (3) 

(3) SPbO + CaCy = 5Pb + Cad 4 2005 

This reaction will take place at higher temperatures, 
while 1 and 2 at lower temperatures. The chloride of Lead re- 
acts in a similar manner. 

(4) PbC1, + CaCp = Pb + CaCl, + 20 


A mixture of the oxide and chloride react according to 


(5) 4Pb0 4 PbClp 4+ CaCn = 5Pb + CaCl, + 2002 

These reactions may be considered as the general re- 
actions of calcium carbide with oxide and chlorides of all of 
the metals named previously. 


Frohlich (4) showed that 1/10 to 1/4 ton of CaCo was 


necessary to produce 1 ton of copper. Kugelgen worked with 


the oxides of fron and CaCo. He was able to get a reduction, 
but claims that it is of no definite value as in the case of 
lead and copper. From what has been discussed so far we can 
represent the reduction of oxides by carbides by two general 
equations: 

(1) 3MO 4+ CaCy CaO + 5M 4+ 2C0 

(2) 5MO 4 CaCy = CaO 4 SM + 2002 

The first takes place with oxides difficultly reduced 
(according to Newmann and Froéhlich). The second with oxides 


easily reduced (Kugelgen). 


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Calcium carbide has been used as a desulphurizing and 


deoxidizing agent in the metallurgical industry mainly in the 


electric furnace where high temperatures are possible. T. M. 


Camp and C. B. Francis in their book, "The Making Shaping and 


Treating of Steel" give the following theory in regards to 


the action and formation of Calcium Carbide in the Heroult 


Furnace. Under the influence of the high temperatures that 


exist around the electrode the CaO and carbon in their vicin- 


ity combine to form calcium carbide. The authors maintain 


that it is at that point when desulphurization takes place. 


The slags of the Heroult furnace contain various amounts of 


free CaCn. The authors claim that a considerable quantity of 


CaCo in the slag is a guarantee that the bath is deoxidized. 


FeO F 
Gace hee) te a7) jy dao’: ace 


3Mn0 Juin 


Moisson (5) did work on the reaction of sulfides with 


calcium carbide. 


FeS + CaC5 = Fe + CaS + 2C 


From the above reactions one can see that CaCog in the 


slag serves as a deoxidizer and desulphurizer. 


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EXPERIMENTAL 


For my experimental work it was necessary to determine 


accurately, the purity of the calcium carbide and iron oxide 


used. The iron oxide was determined by the Permanganate 


method. The CaCy was analyzed by two methods. 


(1) Absorbtion in suprous chloride. 
(2) 


These methods can be combined so that one is a check 


Difference in weight method. 


for the other. The apparatus illustrated below was used. 


%, 


A contains H2504 to ary air passing through apparatus. 


Bis the acetylene generator. 


C a calcium chloride tube. 


Da trap 


E contains a hypochlorite colution for removing sulfur 


and phosphorus. 


F a calcium chloride tube. 


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G and H contain an ammoniacle solution of cuprous 


chloride. 


i Lsxa CaCl, tube. 


The cuprous chloride solution was prepared as given 


in Bloxan. 


30 grams of black copper oxide dissolved in 200 c.c. 


of HCl and boiled for 30 minutes with 24 grams of finely di- 


vided copper. The brown solution is poured into 1750 c.c. of 


H20, allowed to settle, the water drawn off by a siphon and 


the precipitate rinsed into a 1/2 liter bottle. This is 
filled with water and when the ppt. is settled the water is 


drawn off as before. 120 grams of NH,Cl are added and the 


bottle filled with water and shaken. For precipitation this 


solution is poured into 1/10 its bulk of strong ammonia. 


A weighed sample of Calcium Carbide is placed in the 


dry flask B which is fitted with a dropping funnel and delivery 


tubes as indicated. 


A slight excess over the calculated 


amount of water is added. It is best to use a 20% salt (NaCl) 


sOlution as this will reduce the heating effect. B and C are 


carefully weighed (to the third place), G, H and I are also 


weighed. The apparatus is connected to tightly fitting 


rubber tubing. Stop cock o is opened slightly to allow a slow 


stream of dry air to pass through the apparatus. The water 


or salt solution is then allowed to drop very slowly. This 


is necessary or else the gas will pass out unabsorbed. After 


the reaction has stopped, the current of air is allowed to 


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pass through for about 2 hours in order to make sure that 


all of the acetylene has passed into G and H. B and C and 


G, H and I are again weighed. Since, according to the two 


equations, 


(1) CaCe 4 H90 = Ca(OH)g + CoH, 


(2) CoH, + CuCl 4+ eNHs = CucC C Cu + 2NH4Cl 


all of the products remain in the apparatus, the loss 


in weight of B and C should equal the gain in weight of G, H 


and I. The logs in weight of B and © equals the weight of 


CoH> produced, corrected for weight of hydrogen sulfide and 


phosphide evolved. The cuprous acetylide comes down as a red 


precipitate which is insoluble in water. In the analysis, the 


absorption method was omitted. The difference method is 


fairly accurate as will be seen by the results obtained. 


WEIGHT OF WEIGHT OF WEIGHT OF DIFFERENCE “PURE AVERAGE 


CaCo APPARATUS BiC = Wt. of CaCo 
BtC before after CoHa 
23.4837 372.697 368 .450 4.247 44.57 


7.0663 379.011 Ditet io 1.296 44,60 
7.6758 304.470 302.987 1.483 47.29 
(CEPI) 336 .346 334.937 1.409 44.80 45.31 


second Sample 
276.544 274.894 1.650 16S Awe: 
227.698 1.434 78 .60 


5.3568 
4.4914 
Spee | 278.510 276.929 1.581 16.2) 16.79 


229,152 


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The first sample used was very finely divided material 


which had been exposed to the air. For this reason, the 


The second sample was coar- 


sample is rather low in carbide. 


sely ground and only large lusterous lumps of carbide were 


ground, The iron oxide ran 88.6% and 90% pure Fe03. Only 


traces of S were found in either sample. 


FUSIONS 


In order to determine the reaction of Calcium Carbide 


on iron oxide various charges and temperatures were tried. 


The ultimate aim was to reach a temperature condition similar 


For temperatures up to 


to that in the open hearth furnace. 


1250°C a gas furnace was used and above this temperature an 


oil furnace was used. 


Fusion No. I 


A B 
Calo 6.150 grams 5.673 grams 
Fe,0z 15.375 grams 14.182 grams 
C 1 gram 1 gran 


This charge is calculated according to the equation: 


CaCo + Fe50z = 2Fe 4+ CaO 4 2C0 


All figures are based on chemically pure materials. 


The two charges were heated for 3 hours at 1050 to 1100°C. 
In both cases the charges were slightly fused, but did not 


adhere to the crucibles. The fused charges were ground and 


treated for undecomposed CaCp. The charge was placed in B. 


Water was first added, then a dilute solution of HCl, but no 


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acetylene was detected in the cuprous chloride solution. 


Two similar charges were then heated to 1200-1250°C 


for three hours. At this temperature the charges were partly 


fused and adhered to the crucible. On cooling, the upper part 


of the charge contained a grey powder, which on analysis was 


found to be iron. In this case undecomposed carbide was 


analyzed for, but none was detected. The free iron in the 


charge could not be determined as there was present with it 


unreacted Fe0z and perhaps other iron compounds as well. 


In the next flhsions the charges were made up according 


to this equation. 


5Fe503 + 3CaCp = 10Fe + 3Cad + 6C02 


Charges C D E F 
CaCo 5.520 5.438 Spe w)e, 5.401 


Feo03 25.850 25.31 25.00 25.25 


12 grams of slag material of the composition given 


below were added to charges E and F. 


Alj03 - 3 grams 


CaCOz - 5 grams 
NagCOz - 5 grams 
CaF - 5 grams 


5iQ» 12 grams 


These charges were heated to white heat, approximately 


1400°C, for two hours. No attempt was made to pour these 


charges. When removed from the furnace the charges were 


fluid. A glass like slag was produced in all four charges. 


a) 


Rien de ep Mowe Wl gebece ' ' 
eh ag s Asma sida 


oll iy 


11 


Charge C contained a small bead of iron at the bottom weigh- 


ing .2068 grams. Charge E contained a bead weighing 1.253 


grams. No carbide was detected on analysis. From the above 


results it showed that most of the Fe203 went into the slag. 


The addition of slag material produced a larger button. If 


we assume 1.2535 grams, the weight of all the iron reduced in 


charge E, then only 1.789 grams of Fes203 was reduced by the 


carbide. This is a reduction of 7.15% 


The next charges contained the calculated amount of 


Feo93 Plus an excess approximately equivalent to the amount 


that went into the slag in charges ©, D, E and F, The new 


charges were given the same heating and then poured in an iron 


mold. Graphite crucibles were used here instead of the clay 


crucibles. 


Charges 
CaCo used 6.27 6.4 Teer 


Fea03 used 50 50 60 


Wt, of Fe 14,34 26.76 21.03 


% Reduction 28.7 535 35.00 


The above table gives the results obtained in the last 


fusion. The slag in each case could be partly poured. In 


no case was the iron button larger than about 4 grams. The 


slag contained much of the free iron in the form of small 


The slag was broken up to remove the beads of iron. 


beads. 


A strong magnet was used to separate the iron from the slag. 


hc (Se Jae Ress De hake ‘Lema; zt teacoe does ; 


MEbtvoW fied a banda ses 1 Ontas®) + CR 


Ot wft ate ¥i wie nO Datcedeh aa WD + 
j ‘y OTL Jutw ep ee Te igen cai 
edauit Samia be aber Sout dine 
: it Oe te add » 2 
Ul Oi aa oOo athens oe ; 
‘ net <¢ 16 edtabbes 
id Juiupine wild creiie sey: 
esos tl Stele ilge (ied be tea jem 
wt fo lle Gh ot meyer ae ain 
we 4 “Gd deed) Brat go: Nie ty nia BD 
> #1) 30 Lester! trédoteels aay hdd: io 
OTACEME 
i : 
yee he re. 
“rr | ov HE bay 
¢ ite. ‘oe 
J i Deotid@e aie aely ners tee ; w 
ono ofdted: ot Miwon oRag Koay ‘at oat 
scare + Sai aed angel ca vial oe 
50m “TO ptaod see eed ‘pod bom watt ie 


ad ih 


wes Om t ett aaa é a he 


This was added to the iron buttons. Under the conditions of 
the charge and the temperature to which it was heated it is 
not probable that any of the iron that was removed by the 
magnet was magnetite. Any Fez04 formed could react according 
to the equation below. 
Fe,0, +0 = 3FeO + CO 
This reaction takes place at 11759C. The temperature 


of the fusion was about 14009C. From this I conclude that 


there was little or no magnetite formed in the charge. 
Before dissolving the iron a microscopic exanination 


was made of the iron buttons of charges H and I. 


The microphotographs are characteristic of medium 
carbon steel, approximately 45 carbon. The difference in 


structure is due to a change in the rate of cooling. 


> 
pe 
" 


gf) 
oe) ae dale 
aay a) 


CONCLUSIONS 


(1) The results clearly show that when calcium carbide is 
heated in the presence of Fe903 at 1000° a slight reducing 
action takes place. The reaction increases as the tempera- 


ture is increased. Note last results. 


(2) Since no acetylene could be detected when the fused 
charges were treated with water and dilute HCl it seems that 
the carbide is not present as CaC,, but in some form unde- 


termined. 


(3) At temperatures of 1400° and above there is a distinct 


reduction as shown in the data. 


(4) The iron produced is of medium carbon content. Approx- 


imately 0.45%. 


(5) The fluidity of the slag seems to have an apparant e 


effect on the separation of the reduced iron. 


(6) The results clearly show that when CaC2 is added to 
remove sulphur from steel it also reacts as a deoxidi zing 
agent when oxides are present. Whether or not calcium carbide 
is of any commercial value as a reducing agent the writer 
cannot say. The results indicate that there 1s a distinct 
reaction taking place at or neat temperatures maintained in 


an Open hearth furnace. 


Nie a2 A oot) puma 


— 
reine ia 
f . 4 


: iv i/o YR 
gi ‘ fly é | 
re ee, ts ae 


Note: - This thesis represents one semesters work. Had 
more time been devoted, many more results would have 
been obtained and perhaps a much better understanding 


and explanation of the problen. 


? i y i ? 
bin Na aw Pa ey 
— wae, se nnn shee ed aay 


a | 


bed. sto sxotneied eae BY ne ap Ihey tr 


eves! Biwow adletenr CPLOS iaa bedovel’ achat 


ek i allied tet I Ae ate 0 wate ere Lin 
» EE aa a 


‘ea 


BIBLIOGRAPHY 
Ves 2g  meeCus -17 - 177 - 93 
2, Gazetta 1899 29: 509-512 
Bre ee) ies 1901 -T7- 541-550 
557-568 
573-580 


4, Zeitssh. f. Anguvchem 1899 - 1179 
Be ive Oe "Gre 1898 AV | 3355 


TI NERSITY OF ILLINOIS-URBANA 


My 


